CN104497575B - High-thermal-conductivity organosilicone mud and preparation method thereof - Google Patents

High-thermal-conductivity organosilicone mud and preparation method thereof Download PDF

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CN104497575B
CN104497575B CN201410822370.3A CN201410822370A CN104497575B CN 104497575 B CN104497575 B CN 104497575B CN 201410822370 A CN201410822370 A CN 201410822370A CN 104497575 B CN104497575 B CN 104497575B
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silicone oil
mud
heat conduction
powder
conductivity
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CN104497575A (en
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张震宇
陈思斌
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Guangzhou Baiyun Technology Co ltd
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Guangzhou Baiyun Chemical Industry Co Ltd
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Abstract

The invention discloses a high-thermal-conductivity organosilicone mud. The high-thermal-conductivity organosilicone mud is prepared from the following raw materials: 100 parts of silicone oil and 1000-1200 parts of heat-conducting powder filler in parts by weight, 0.5-1wt% of plasticizer and 1-3wt% of powder surface treating agent in terms of the heat-conducting powder filler, and 1-3wt% of cross-linking agent, 5-10wt% of high temperature resistant pigment and 0.01-0.015wt% of platinum catalyst in terms of the silicone oil. Besides, the invention also discloses a preparation method of the high-thermal-conductivity organosilicone mud. The high-thermal-conductivity organosilicone mud product has the advantages of high thermal conductivity, stable heat transfer property, excellent high temperature resistance, plasticity just as plasticine and the like; the preparation method of the high-thermal-conductivity organosilicone mud is simple; a better thermal-conductivity solution way can be provided for electronic heating components and radiating or other cooling devices.

Description

A kind of organosilicon high heat conduction mud and preparation method thereof
Technical field
The present invention relates to conduction heat transfer technical field, more particularly to a kind of organosilicon high heat conduction mud and preparation method thereof.
Background technology
Increasingly strict, the electronic product function of requiring with the fast development of Manufacturing science technology and to properties of product The stability for using is faced with the market test of sternness, how to solve the problems, such as that equipment cooling has become the whole machine miniaturization of electronic product The key of design.Because air conduction is poor, if the heat that equipment is generated shed not in time, local is easily formed high Temperature, and high temperature can cause electronic component to puncture arcing etc., and then cause to damage components and parts and component, so as to affect electronic product Reliability and normal work usage cycles.For this purpose, in the design and fabrication of electronic product, in order to chip etc. is generated heat first device The heat that part is produced sheds, it will usually interface Heat Conduction Material is used between radiator and the components and parts of heating, with time by heat Amount is dissipated, so as to ensure the stable normal operation of equipment.
Traditional interface Heat Conduction Material is heat-conducting silicone grease, is typically with the extremely low silicone oil of viscosity and leads to conduction powder filler Cross mechanical strong stirring to mix, this material almost never solidifies.Heat-conducting silicone grease has excellent electrical insulating property, heat conduction The performance such as property, high-low temperature resistant, water-fast, ozone, weather-resistant.However, because the density of conduction powder filler is far longer than silicon The density of oil, oil meal is easily separated, therefore prior art also takes the method by being processed conduction powder filler, To improve settlement issues, but effect is not apparent.Especially during the life-time service when temperature is more than 80 DEG C, lead Silicone oil in hot silicone grease slowly can dissociate, and split and air inlet so as to cause thermal conductive silicon lipid layer to be dried so that heat transfer is stable Property be deteriorated, had a strong impact on the usage cycles of electronic product equipment.
With the fast development of the whole machine miniaturization of electronic product and high-power, heat generating component temperature is constantly raised, ground System exploitation has high thermal conductivity, stable heat transfer property, superior resistance to elevated temperatures, oil-tight, non-volatile, usage cycles length Organosilicon heat conduction product has become the direction and emphasis studied in the industry.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of heat conductivility is stable, without permeability, use when Between long and with good adhesion and excellent heat conducting efficiency organosilicon high heat conduction mud, be electronic heating components and parts and radiating or More preferable heat conduction solution route is provided between other cooling devices.Another object of the present invention is to provide above-mentioned organosilicon height lead The preparation method of warm sludge.
The purpose of the present invention is achieved by the following technical programs:
A kind of organosilicon high heat conduction mud that the present invention is provided, its raw material is consisted of:Silicone oil, conduction powder filler, plasticizer, Surface treatment agent for powder, cross-linking agent, high temperature resistant colorant, platinum catalyst;According to parts by weight silicone oil be 100 parts, conduction powder fills out Expect for 1000~1200 parts;In terms of conduction powder filler, plasticizer consumption be 0.5~1wt%, the consumption of surface treatment agent for powder For 1~3wt%;In terms of silicone oil, the consumption of cross-linking agent is 1~3wt%, and the consumption of high temperature resistant colorant is 5~10wt%, platinum catalysis The consumption of agent is 0.1~0.15wt ‰.
Further, silicone oil of the present invention is phenyl-vinyl silicon oil, and viscosity is 300~1000cp.The conductive powder Body filler be aluminium oxide, Zinc Oxide, boron nitride, carborundum, aluminium nitride powder in one kind or its combination, its particle diameter be 0.5~ 10 μm, grain shape is ball-type.The plasticizer is methyl-silicone oil, and viscosity is 100~500cp.The surface treatment agent for powder For the one kind in long chain alkyl silane, titanate esters, hard fatty acids or its combination.The cross-linking agent is that end containing hydrogen silicone oil and side chain contain The mixture of hydrogen silicone oil;Specially according to mol ratio end containing hydrogen silicone oil: side chain containing hydrogen silicone oil=7: 3 mixture, after compounding Viscosity is 10~50cp, wherein, the structural formula of the end containing hydrogen silicone oil is H-Si (CH3)2-O-[Si(CH3)2-O]n-Si (CH3)2- H, the structural formula of the side chain containing hydrogen silicone oil is C3H9-Si-O-[Si(CH3)(H)-O]n-Si-C3H9.The high temperature resistant Colorant is cobalt blue, barba hispanica or titanium blue.The platinum catalyst is Karst platinum catalyst.
Another object of the present invention is achieved by the following technical programs:
The preparation method of the above-mentioned organosilicon high heat conduction mud that the present invention is provided, comprises the following steps:First by silicone oil with lead Hot powder stuffing is uniformly mixed under the conditions of vacuum protection, then sequentially add in batches plasticizer, surface treatment agent for powder, Cross-linking agent, high temperature resistant colorant, platinum catalyst, are warming up to 55~65 DEG C under the conditions of vacuum protection, react 0.5~2h, are cooled to Room temperature obtains organosilicon high heat conduction mud finished product.
The invention has the advantages that:
(1) in inventive formulation system, silicone oil forms spatial networks crosslinking with cross-linking agent, by conduction powder filler securely Parcel wherein, so as to ensure that resin and conduction powder filler are difficult layering, is prevented because conduction powder packing density is too big Caused sedimentation so that product has the excellent characteristics such as oil-tight, non-volatile, storage cycle length.Also, at powder surface Reason agent is surface-treated to conduction powder filler, eliminates powder surface such as hydroxyl or other reactive polar groups, reduces Molecular force (such as hydrogen bond) between powder granule, is substantially increased the loading of conduction powder filler, effectively Ensure that the high thermal conductivity of product.Additionally, by formulas optimized design, using the conduction powder filler and Nai Gao of consumption at high proportion Warm colour material, improves the resistance to elevated temperatures of product so as under 200 DEG C of hot conditionss can with the performance of stable for extended periods of time, Can avoid what is significantly declined similar to the heat transfer property caused by silicone oil vaporization at high temperature in prior art heat-conducting silicone grease Problem.
(2) organosilicon high heat conduction mud of the present invention is the plasticity jelly similar to plasticine, so as to increased its construction Method (in addition to conventional brushing and silk screen printing, can also adopt modularity), and easy construction is flexible.Meanwhile, product has Certain elasticity, can effectively eliminate the internal stress that heat generating component is produced due to vibration, so as to ensure good heat-conducting effect, can Play the effect such as high heat conduction, insulation, dust-proof, moistureproof, shockproof.
(3) organosilicon high heat conduction mud product of the present invention has stable, the superior heat-resisting quantity of thermal conductivity height, heat transfer property Can, oil-tight, non-volatile and plasticity similar to plasticine the advantages of, preparation process is simple can be electronic heating unit Between the assembling (such as radiator accessories and Led chip aluminium bases) of device and heating element and radiating or other cooling devices More preferable heat conduction solution route is provided, can be widely applied to high power module, integrated chip, power module, auto electronic product, The radiating of the heating elements such as controller, communication apparatus, computer and its adnexa.
Below in conjunction with embodiment, the present invention is described in further detail.
Specific embodiment
A kind of organosilicon high heat conduction mud of the embodiment of the present invention, its raw material is consisted of:Silicone oil, conduction powder filler, plasticizer, Surface treatment agent for powder, cross-linking agent, high temperature resistant colorant, platinum catalyst.Wherein, silicone oil is phenyl-vinyl silicon oil, and viscosity is 300 ~1000cp;Conduction powder filler is one kind or its group in aluminium oxide, Zinc Oxide, boron nitride, carborundum, aluminium nitride powder Close;Plasticizer is methyl-silicone oil, and viscosity is 100~500cp;Surface treatment agent for powder is long chain alkyl silane, titanate esters, Hard Fat One kind or its combination in fat acid;Cross-linking agent is according to mol ratio end containing hydrogen silicone oil: side chain containing hydrogen silicone oil=7: 3 mixture, Viscosity after compounding is 10~50cp, wherein, the structural formula for holding containing hydrogen silicone oil is H-Si (CH3)2-O-[Si(CH3)2-O]n-Si (CH3)2- H, the structural formula of side chain containing hydrogen silicone oil is C3H9-Si-O-[Si(CH3)(H)-O]n-Si-C3H9;High temperature resistant colorant is cobalt Blue, barba hispanica or titanium blue;Platinum catalyst is Karst platinum catalyst.It is specific as follows:
Embodiment one:
1st, a kind of organosilicon high heat conduction mud of the present embodiment, its raw material is consisted of:
2nd, the preparation method of the above-mentioned organosilicon high heat conduction mud of the present embodiment, its step is as follows:
Add phenyl-vinyl silicon oil in planet machine first, conduction powder filler is sequentially added in five batches ,- It is uniformly mixed under the conditions of the vacuum protection of 0.095MPa;Then plasticizer, surface treatment agent for powder, crosslinking are sequentially added Agent, high temperature resistant colorant, platinum catalyst, are warming up to 65 DEG C of reaction 0.5h under the conditions of the vacuum protection of -0.095MPa, are cooled to room Temperature obtains organosilicon high heat conduction mud finished product.
Embodiment two:
1st, a kind of organosilicon high heat conduction mud of the present embodiment, its raw material is consisted of:
2nd, the preparation method of the above-mentioned organosilicon high heat conduction mud of the present embodiment, its step is as follows:
Add phenyl-vinyl silicon oil in planet machine first, conduction powder filler is sequentially added in five batches ,- It is uniformly mixed under the conditions of the vacuum protection of 0.095MPa;Then plasticizer, surface treatment agent for powder, crosslinking are sequentially added Agent, high temperature resistant colorant, platinum catalyst, are warming up to 60 DEG C of reaction 1h under the conditions of the vacuum protection of -0.095MPa, are cooled to room temperature Obtain organosilicon high heat conduction mud finished product.
Embodiment three:
1st, a kind of organosilicon high heat conduction mud of the present embodiment, its raw material is consisted of:
2nd, the preparation method of the above-mentioned organosilicon high heat conduction mud of the present embodiment, its step is as follows:
Add phenyl-vinyl silicon oil in planet machine first, conduction powder filler is sequentially added in six batches ,- It is uniformly mixed under the conditions of the vacuum protection of 0.095MPa;Then plasticizer, surface treatment agent for powder, crosslinking are sequentially added Agent, high temperature resistant colorant, platinum catalyst, are warming up to 55 DEG C of reaction 2h under the conditions of the vacuum protection of -0.095MPa, are cooled to room temperature Obtain organosilicon high heat conduction mud finished product.
The physical and chemical performance index of organosilicon high heat conduction mud finished product prepared by various embodiments of the present invention is as shown in table 1 below.
The physical and chemical performance index of organosilicon high heat conduction mud finished product prepared by the various embodiments of the present invention of table 1
A kind of organosilicon high heat conduction mud of the present invention and preparation method thereof, its raw material composition and preparation method technological parameter are not It is confined to the above-mentioned embodiment enumerated.

Claims (5)

1. a kind of organosilicon high heat conduction mud, it is characterised in that raw material is consisted of:Silicone oil, conduction powder filler, plasticizer, powder body table Face inorganic agent, cross-linking agent, high temperature resistant colorant, platinum catalyst;According to parts by weight silicone oil be 100 parts, conduction powder filler be 1000~1200 parts;In terms of conduction powder filler, plasticizer consumption is 0.5~1wt%, and the consumption of surface treatment agent for powder is 1 ~3wt%;In terms of silicone oil, the consumption of cross-linking agent is 1~3wt%, and the consumption of high temperature resistant colorant is 5~10wt%, platinum catalyst Consumption be 0.1~0.15wt ‰;
The silicone oil is phenyl-vinyl silicon oil, and viscosity is 300~1000cp;
The surface treatment agent for powder is the one kind in octadecyl trimethoxysilane, titanate esters, hard fatty acids or its combination;
The plasticizer is methyl-silicone oil, and viscosity is 100~500cp;
The cross-linking agent is the mixture for holding containing hydrogen silicone oil and side chain containing hydrogen silicone oil, according to mol ratio end containing hydrogen silicone oil: side chain contains Hydrogen silicone oil=7: 3 mixture, the viscosity after compounding is 10~50cp, wherein, the structural formula of the end containing hydrogen silicone oil is H-Si (CH3)2-O-[Si(CH3)2-O]n-Si(CH3)2- H, the structural formula of the side chain containing hydrogen silicone oil is C3H9-Si-O-[Si(CH3) (H)-O]n-Si-C3H9
2. organosilicon high heat conduction mud according to claim 1, it is characterised in that:The conduction powder filler be aluminium oxide, One kind or its combination in Zinc Oxide, boron nitride, carborundum, aluminium nitride powder, its particle diameter is 0.5~10 μm, and grain shape is Ball-type.
3. organosilicon high heat conduction mud according to claim 1, it is characterised in that:The high temperature resistant colorant is cobalt blue, barba hispanica Or titanium blue.
4. organosilicon high heat conduction mud according to claim 1, it is characterised in that:The platinum catalyst is Karst platinum catalysis Agent.
5. the preparation method of one of claim 1-4 organosilicon high heat conduction mud, it is characterised in that comprise the following steps:First Silicone oil is uniformly mixed with conduction powder filler under the conditions of vacuum protection, plasticizer, powder body are then sequentially added in batches Surface conditioning agent, cross-linking agent, high temperature resistant colorant, platinum catalyst, are warming up to 55~65 DEG C, reaction 0.5 under the conditions of vacuum protection ~2h, is cooled to room temperature and obtains organosilicon high heat conduction mud finished product.
CN201410822370.3A 2014-12-22 2014-12-22 High-thermal-conductivity organosilicone mud and preparation method thereof Active CN104497575B (en)

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RU2612677C2 (en) * 2015-06-15 2017-03-13 Общество с ограниченной ответственностью "Новая Химия" Plastic silicone composition with bulk filler
CN105566920A (en) * 2015-12-24 2016-05-11 平湖阿莱德实业有限公司 Low-oil-permeability super-soft thermally-conductive silica gel composition and thermally-conductive silica gel gasket and preparation method thereof
CN106085252A (en) * 2016-06-21 2016-11-09 北京派诺蒙能源科技有限公司 A kind of heat-conducting daub and its preparation method and application
CN108513495B (en) * 2016-08-26 2019-07-16 浙江大学 A kind of board radiator heat conducting gum mud pressure setting
CN106700555A (en) * 2017-01-18 2017-05-24 东莞市新懿电子材料技术有限公司 High thermal conductive silicone grease and preparation method thereof
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CN107141815B (en) * 2017-06-24 2020-03-24 肇庆皓明有机硅材料有限公司 High-temperature-resistant low-modulus heat-conducting organosilicon material and preparation method thereof
CN108440968A (en) * 2018-03-27 2018-08-24 董小琳 A kind of high heat conduction silicon aluminum nitrides rubber cushion and preparation method thereof
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CN109401319A (en) * 2018-09-04 2019-03-01 苏州泰吉诺新材料科技有限公司 A kind of long-acting thermostable heat-conductive silicone grease and preparation method thereof
CN111560187A (en) * 2019-11-26 2020-08-21 东莞市美庆电子科技有限公司 Heat conduction mud and preparation method thereof
CN110903656B (en) * 2019-11-28 2022-05-17 华南协同创新研究院 Low-volatility temperature-resistant heat-conducting silica gel cement material and preparation method and application thereof
CN113248931A (en) * 2021-05-31 2021-08-13 广东恒大新材料科技有限公司 Heat-conducting gel with high heat conductivity and high extrusion rate and preparation method thereof
CN115404051A (en) * 2022-09-24 2022-11-29 宁波聚力新材料科技有限公司 High-thermal-conductivity easily-molded heat-conducting mud and preparation method thereof

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Address after: Guangzhou private science and Technology Park Yunan road Baiyun District of Guangzhou City, Guangdong Province, No. 1 510540

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